SW-846 Update V 3511 - 1 Revision 1 

October 2012 

METHOD 3511 

 ORGANIC COMPOUNDS IN WATER BY MICROEXTRACTION 

SW-846 is not intended to be an analytical training manual. Therefore, method procedures 

are written based on the assumption that they will be performed by analysts who are formally 

trained in at least the basic principles of chemical analysis and in the use of the subject 

technology. 

In addition, SW-846 methods, with the exception of required method use for the analysis of 

method-defined parameters, are intended to be guidance methods which contain general 

information on how to perform an analytical procedure or technique which a laboratory can use as 

a basic starting point for generating its own detailed standard operating procedure (SOP), either 

for its own general use or for a specific project application. The performance data included in this 

method are for guidance purposes only, and are not intended to be and must not be used as 

absolute QC acceptance criteria or for the purpose of laboratory accreditation. 

1.0 SCOPE AND APPLICATION 

For a summary of changes in this version, please see Appendix A at the end of this 

document. 

1.1 Method 3511 is a procedure for extracting selected volatile and semivolatile 

organic compounds from water. The microscale approach minimizes sample size and solvent 

usage, thereby reducing the supply costs, health and safety risks, and waste generated. 

1.2 This method was validated for several mono- and poly-cyclic aromatic 

hydrocarbons (MAHs and PAHs) and can be applied to any combination of these compounds. 

1.3 This method also may be used to extract selected volatile organic compounds 

(VOCs) or semivolatile organic compounds (SVOCs) which are slightly soluble or insoluble in 

water at neutral pH if the extraction performance is demonstrated to be satisfactory using an 

appropriate analytical technique. 

1.4 Prior to employing this method, analysts are advised to consult the base method 

for each type of procedure that may be employed in the overall analysis (e.g., Methods 3500, 

3600, 5000, and 8000) for additional information on quality control procedures, development of 

QC acceptance criteria, calculations, and general guidance. Analysts also should consult the 

disclaimer statement at the front of the manual and the information in Chapter Two for guidance 

on the intended flexibility in the choice of methods, apparatus, materials, reagents, and supplies, 

and on the responsibilities of the analyst for demonstrating that the techniques employed are 

appropriate for the analytes of interest, in the matrix of interest, and at the levels of concern. 

In addition, analysts and data users are advised that, except where explicitly required in a 

regulation, the use of SW-846 methods is not mandatory in response to Federal testing 

requirements. The information contained in this method is provided by EPA as guidance to be 

used by the analyst and the regulated community in making judgments necessary to generate 

results that meet the data quality objectives for the intended application. 

1.5 Use of this method is restricted to use by, or under supervision of, appropriately 

experienced and trained personnel. Each analyst must demonstrate the ability to generate 

acceptable results with this method. 
SW-846 Update V 3511 - 2 Revision 1 

October 2012 

2.0 SUMMARY OF METHOD 

2.1 Samples are prepared by liquid:liquid extraction with organic solvent in field 

sampling containers. Careful manipulation of the sample, solvent, and spiking solutions during 

the procedure minimizes loss of volatile compounds while maximizing extraction of volatile, 

semivolatile, and nonvolatile compounds. 

2.2 Since volatile compounds are included in the method, their extraction from water 

requires special handling and particular attention to detail. Samples should be removed from the 

refrigerator shortly before extraction, and should not be allowed to warm to room temperature 

before the extraction solvent is added. 

2.3 Samples should be prepared one at a time to the point of solvent addition (i.e., do 

not prepare a number of samples then add the solvent). Pay particular attention to minimizing 

the exposure of the sample and/or extract to air. 

2.4 Determinative analysis is performed using the appropriate GC or GC/MS method 

(e.g., 8015, 8021 and 8270). Reference 2 shows an example of a GC configuration used for the 

entire list of target analytes that may help reduce solvent tailing to prevent interference with any 

early-eluting target compounds in this method. 

3.0 DEFINITIONS 

Refer to the SW-846 chapter of terms and acronyms for potentially applicable definitions. 

4.0 INTERFERENCES 

4.1 Solvents, reagents, glassware, and other sample processing hardware may yield 

artifacts and/or interferences to sample analysis. All of these materials must be demonstrated to 

be free from interferences under the conditions of the analysis by analyzing method blanks. 

Specific selection of reagents and purification of solvents by distillation in all-glass systems may 

be necessary. Refer to each method for specific guidance on quality control procedures and to 

Chapter Four for general guidance on the cleaning of glassware. 

4.2 Refer to Method 3500 for additional information on interferences. 

5.0 SAFETY 

There are no significant safety issues specific to this method. However, SW-846 

methods do not purport to address all safety issues associated with their use. The laboratory is 

responsible for maintaining a safe work environment and a current awareness file of OSHA 

regulations regarding the safe handling of the chemicals listed in this method. A reference file of 

material safety data sheets (MSDSs) should be available to all personnel involved in these 

analyses. 
SW-846 Update V 3511 - 3 Revision 1 

October 2012 

6.0 EQUIPMENT AND SUPPLIES 

The mention of trade names or commercial products in this manual is for illustrative 

purposes only, and does not constitute an EPA endorsement or exclusive recommendation for 

use. The products and instrument settings cited in SW-846 methods represent those products 

and settings used during method development or subsequently evaluated by the Agency. 

Glassware, reagents, supplies, equipment, and settings other than those listed in this manual 

may be employed provided that method performance appropriate for the intended application has 

been demonstrated and documented. 

6.1 VOA vials - 40-mL capacity, disposable, pre-cleaned with 

Polytetrafluoroethylene (PTFE)-lined caps 

6.2 Vials - Amber glass, 2-mL capacity, with PTFE-lined screw or crimp top 

6.3 Centrifuge - Capable of at least 500 G’s 

6.4 Syringes - gastight, contaminant-free, 2.0-mL, 1.0-mL, 10-μL 

6.5 Analytical balance - Capable of weighing to 0.01 g 

6.6 Pasteur glass pipettes - 1mL, disposable 

7.0 REAGENTS AND STANDARDS 

7.1 Reagent grade chemicals must be used in all tests. Unless otherwise indicated, 

it is intended that all reagents conform to the specifications of the Committee on Analytical 

Reagents of the American Chemical Society, where such specifications are available. Other 

grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to 

permit its use without lessening the accuracy of the determination. 

7.2 Organic-free reagent water. All references to water in this method refer to 

organic-free reagent water as defined in Chapter One. 

 7.3 Sodium sulfate (granular, anhydrous), Na2SO4. Purify by heating at 400 °C for 

four hours in a shallow porcelain bowl. Store unused portion of sodium sulfate in a desiccator or 

sealed container. 

7.4 Extraction and exchange solvents 

The choice of solvent will depend on the analytes of interest and no single solvent is 

universally applicable to all analyte groups. Whatever solvent system is employed including

those specifically listed in this method, the analyst must demonstrate adequate performance for 

the analytes of interest, at the levels of interest. At a minimum, such a demonstration will 

encompass the initial demonstration of proficiency described in Method 3500, using a clean 

reference matrix. Method 8000 describes procedures that may be used to develop performance 

criteria for such demonstrations as well as for matrix spike and laboratory control sample results. 

All solvents should be pesticide quality or equivalent. Solvents may be degassed prior to 

use. 

 7.4.1 Methylene chloride, CH2Cl2. 
SW-846 Update V 3511 - 4 Revision 1 

October 2012 

8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 

See the introductory material to this chapter, Organic Analytes, Sec. 4.1. 

Samples should be extracted as soon as after collection as possible, but no longer than 14 

days from the date of collection for acid preserved samples. If samples are not acidified, the 

extraction should be performed within 7 days from date of collection. 

9.0 QUALITY CONTROL 

9.1 Refer to Chapter One for guidance on quality assurance (QA) and quality control 

(QC) protocols. When inconsistencies exist between QC guidelines, method-specific QC criteria 

take precedence over both technique-specific criteria and the criteria given in Chapter One, and 

technique-specific QC criteria take precedence over the criteria in Chapter One. Any effort 

involving the collection of analytical data should include development of a structured and 

systematic planning document, such as a Quality Assurance Project Plan (QAPP) or a Sampling 

and Analysis Plan (SAP), which translates project objectives and specifications into directions for 

those that will implement the project and assess the results. Each laboratory should maintain a 

formal quality assurance program. The laboratory should also maintain records to document the 

quality of the data generated. All data sheets and quality control data should be maintained for 

reference or inspection. 

 

9.2 Initial demonstration of proficiency and lower limit of quantitation (LLOQ) 

Each laboratory must demonstrate initial proficiency with each sample preparation and 

determinative method combination it utilizes by generating data of acceptable accuracy and 

precision for target analytes in a clean matrix. The laboratory must also repeat the 

demonstration of proficiency whenever new staff members are trained or significant changes in 

instrumentation are made. See Method 8000D, Sec. 9.3 for information on how to accomplish a 

demonstration of proficiency. 

The laboratory shall establish the LLOQ as the lowest point of quantitation, which in most 

cases, is the lowest concentration in the calibration curve. LLOQ verification is recommended 

for each project application to validate quantitation capability at low analyte concentration levels. 

This verification may be accomplished with either clean control material (e.g., reagent water, 

solvent blank, Ottawa sand, diatomaceous earth, etc.) or a representative sample matrix, free of 

target compounds. Optimally, the LLOQ should be less than the desired regulatory action levels 

based on the stated DQOs. 

In order to demonstrate the entire sample preparation and analysis process at the lower 

limit of quantitation (LLOQ), a LLOQ check standard (not part of an initial calibration) is prepared 

by spiking a clean control material with the analyte(s) of interest at the predicted LLOQ 

concentration level(s). Alternatively, a representative sample matrix may be spiked with the 

analytes of interest at the predicted LLOQ concentration levels. The LLOQ check is carried 

through the same preparation procedures as environmental samples and other QC samples. 

Recovery of target analytes in the LLOQ check standard should be within established 

in-house limits, or other such project-specific acceptance limits, to demonstrate acceptable 

method performance at the LLOQ. Until the laboratory has sufficient data to determine 

acceptance limits, the LCS criteria ± 20% may be used for the LLOQ acceptance criteria. This 
SW-846 Update V 3511 - 5 Revision 1 

October 2012 

acknowledges the poorer overall response at the low end of the calibration curve. 

Historically-based LLOQ acceptance criteria should be determined as soon as practical once 

sufficient data points have been acquired. 

9.4 Refer to Method 3500 for additional quality control procedures. 

9.5 Before processing any samples, the analyst should demonstrate that all parts of 

the equipment in contact with the sample and reagents are interference-free. This is 

accomplished through the analysis of a method blank. Each time samples are extracted, 

cleaned up, and analyzed, and when there is a change in reagents, a method blank should be 

prepared and analyzed for the compounds of interest as a safeguard against chronic laboratory 

contamination. 

 

9.6 Any method blanks, matrix spike samples, or replicate samples should be 

subjected to the same analytical procedures (Sec. 11.0) as those used on actual samples. 

9.7 Each extraction batch of twenty or fewer samples should include a minimum of a 

method blank, a laboratory control sample (LCS), a matrix spike sample, and a matrix spike 

duplicate or laboratory duplicate sample. 

9.8 All field and QC samples should be spiked with an appropriate mix of surrogate 

compounds in order to track extraction efficiency. 

9.9 Any QC samples should be subjected to exactly the same analytical procedures 

as those used on field samples. 

10.0 CALIBRATION AND STANDARDIZATION 

There are no calibration or standardization steps directly associated with this extraction 

procedure. 

11.0 PROCEDURE 

 Refer to Sec. 9 for a list of number and types of QC samples that should be included with 

each batch of 20 or fewer field samples. 

 11.1 For each QC sample to be extracted and analyzed, prepare one vial as described 

below (Sec. 11.3). 

11.2 If volatile compounds are target analytes of interest, the QC vials must be 

prepared far enough in advance that the water has time to chill before extraction. However, 

these vials should not be allowed to sit in the refrigerator for more than 24 hours, or their integrity 

may be suspect. 

11.3 For each method blank or LCS QC sample, fill a 40 mL glass VOA vial with a 

PTFE-lined septum screw top with reagent water. 

11.4 If volatile compounds are target analytes of interest, make sure that all field and 

QC samples are chilled to less than 4°C before proceeding. 
SW-846 Update V 3511 - 6 Revision 1 

October 2012 

11.5 Working with a single field or QC sample at a time, remove the cap from the VOA 

vial, and use a disposable pipette to remove approximately 5 mL of water. Alternatively, remove 

enough sample volume from the vial to prevent vessel overflow, however, too much volume 

removed will create a potential for headspace and loss of volatile constituents. In addition, the 

amount of time used to process volatile compound extracts up to the point of solvent addition 

needs to be kept to a minimum in order to avoid further volatile constituent losses. Replace the 

vial cap. 

 

The volume removed should be disposed of according to the guidelines set forth by the 

laboratory for the disposal of laboratory wastes. 

11.6 After removing the 5 mL, weigh the capped VOA vial for each field and QC 

sample. Record the weight to the nearest 0.1 grams. 

11.7 Remove the cap and add 10 μg of the surrogate standard compounds in acetone. 

The surrogates recommended are fluorobenzene, 2-fluorobiphenyl, and 5-a-androstane. Other 

compounds may be used as surrogates, depending upon the desired target analytes and project 

requirements. 

11.7.1 It should be noted that more surrogate standard may be added to the 

water if the sample is suspected to be highly contaminated (i.e., the contamination may 

interfere with the recovery of lower concentration levels of surrogate standard). 

11.7.2 The LCS and matrix spike QC samples should have 10 μg of the 

appropriate compounds of interest added. 

11.8 Add exactly 2.0 mL of methylene chloride (DCM) (using a class A volumetric 

pipette or gas-tight syringe) and approximately 12 g of anhydrous sodium chloride to the VOA vial. 

Replace the vial cap. At this point, the next sample may be processed to the point of solvent 

addition and the subsequent steps performed for each sample batch. 

11.9 Shake each vial vigorously for 5 minutes, or until the sodium chloride dissolves 

completely. 

11.10 Allow the phases to separate. Centrifugation may be useful for separating the 

phases. If the emulsion interface between layers is more than one-third the size of the solvent 

layer, the analyst should employ mechanical techniques to complete the phase separation. The 

optimum technique depends upon the sample and may include stirring, filtration of the emulsion 

through glass wool, centrifugation, or other physical methods. 

11.11 Using a 2.0-mL gas-tight syringe, transfer approximately 1.5 mL of the lower 

(DCM) layer to a 2 mL vial fitted with a PTFE lined screw cap, taking precautions to exclude any 

water from the syringe. Add a small amount (~50 mg) of anhydrous sodium sulfate to the vial, 

cap, and shake for 2 minutes. 

11.12 Using a 1.0 mL gas-tight syringe, transfer exactly 1.0 mL of the dried extract to a 

2 mL vial fitted with a PTFE lined screw cap. Add 50 μg of the internal standard compounds to 

each vial, using an appropriate volume not to overflow the vial or dilute the extract. The internal 

standards recommended are o-terphenyl and 2,4-difluorotoluene. Other compounds may be 

used as internal standards, depending upon the desired target analytes and project requirements. 

Cap the vial and invert several times to mix the contents. 
SW-846 Update V 3511 - 7 Revision 1 

October 2012 

11.13 Discard the remaining contents of the VOA vials according to laboratory waste 

disposal guidelines. Shake off the last few drops with short, brisk wrist movements. If needed, 

rinse the vial with a water soluble solvent to ensure that the extraction solvent is removed. 

Reweigh the capped vial, and record the weight to the nearest 0.1 g. The difference between 

this weight, and the weight determined in Sec. 11.6 is equal to the volume of water extracted, in 

mL. 

11.14 Extracts should be stored in the freezer or over ice until analysis. 

12.0 DATA ANALYSIS AND CALCULATIONS 

 There are no data analysis and calculation steps directly associated with this procedure. 

Follow the directions given in the determinative method. 

13.0 METHOD PERFORMANCE 

13.1 Performance data and related information are provided in SW-846 methods only 

as examples and guidance. The data do not represent required performance goals for users of 

the methods. Instead, performance criteria should be developed on a project-specific basis, and 

the laboratory should establish in-house QC performance criteria for the application of this 

method. 

13.2 Single-laboratory precision data were obtained for MAHs and PAHs at four 

different spiking concentrations in reagent water. Three replicates were prepared at three levels, 

and six replicates at one level. Extracts were analyzed by Method 8100, set up to include the 

MAHs along with the PAHs. Data summary tables are included in this method. For guidance 

purposes, the data are reported in detail in Reference 1. 

14.0 POLLUTION PREVENTION 

14.1 Pollution prevention encompasses any technique that reduces or eliminates the 

quantity and/or toxicity of waste at the point of generation. Numerous opportunities for pollution 

prevention exist in laboratory operations. The EPA has established a preferred hierarchy of 

environmental management techniques that places pollution prevention as the management 

option of first choice. Whenever feasible, laboratory personnel should use pollution prevention 

techniques to address their waste generation. When wastes cannot be feasibly reduced at the 

source, the Agency recommends recycling as the next best option. 

14.2 For information about pollution prevention that may be applicable to laboratories and 

research institutions consult Less is Better: Laboratory Chemical Management for Waste 

Reduction, a free publication available from the American Chemical Society (ACS), Committee on 

Chemical Safety, http://portal.acs.org/portal/fileFetch/C/WPCP_012290/pdf/WPCP_012290.pdf. 

15.0 WASTE MANAGEMENT 

The Environmental Protection Agency requires that laboratory waste management 

practices be conducted consistent with all applicable rules and regulations. The Agency urges 

laboratories to protect the air, water, and land by minimizing and controlling all releases from 

hoods and bench operations, complying with the letter and spirit of any sewer discharge permits 
SW-846 Update V 3511 - 8 Revision 1 

October 2012 

and regulations, and by complying with all solid and hazardous waste regulations, particularly the 

hazardous waste identification rules and land disposal restrictions. For further information on 

waste management, consult The Waste Management Manual for Laboratory Personnel available 

from the American Chemical Society at the address listed in Sec. 14.2. 

16.0 REFERENCES 

1. "Simultaneous Analysis of Monocyclic Aromatic Hydrocarbons in Water by 

Microextraction." EPRI Report TR-Research Project, April 1997. 

2. D. M. Munro. “Simultaneous Determination of Volatile and Semivolatile Organic 

Compounds in Soil.” Remediation Journal, 10, pp. 65-81, 2000. 

http://onlinelibrary.wiley.com/doi/10.1002/rem.3440100408/pdf 

17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA 

The following pages contain the tables referenced by this method. 
SW-846 Update V 3511 - 9 Revision 1 

October 2012 

TABLE 1 

 EXAMPLE MICROEXTRACTION GC/FID RECOVERY DATA FOR 

 MAHs AND PAHs IN REAGENT WATER SPIKED AT 8.57 μg/L1

Compound 

Sample A Sample B Sample C Std. 

Dev. 

Conc.2 % Rec. Conc.2 % Rec. Conc.2 % Rec. (Conc.2)

Benzene 9.59 112 7.40 86 8.80 103 1.1

Toluene 9.03 105 9.44 110 9.36 109 0.22

Ethylbenzene 8.60 100 8.81 103 8.87 103 0.14

m/p-Xylene 17.0 99 18.1 106 18.1 106 0.60

Styrene 6.86 80 7.17 84 6.99 82 0.16

o-Xylene 9.94 116 10.3 120 10.5 123 0.31

1,2,4-Trimethylbenzene 7.44 87 8.53 100 8.35 97 0.59

Naphthalene 7.02 82 7.36 86 7.48 87 0.24

2-Methylnaphthalene 7.11 83 7.76 91 7.96 93 0.45

1-Methylnaphthalene 7.98 93 8.45 99 8.80 103 0.41

Acenaphthylene 8.44 98 8.45 99 8.74 102 0.17

Acenaphthene 9.23 108 9.73 114 9.61 112 0.26

Dibenzofuran 6.72 78 7.01 82 6.99 82 0.16

Fluorene 6.17 72 6.62 77 7.35 86 0.60

Phenanthrene 7.43 87 7.90 92 7.74 90 0.24

Anthracene 4.76 56 6.19 72 6.24 73 0.84

Fluoranthene 8.12 95 8.53 100 8.57 100 0.25

Pyrene 8.49 99 8.78 102 8.92 104 0.22

Benz(a)anthracene 6.59 77 6.88 80 6.46 75 0.21

Chrysene 5.78 67 5.92 69 6.14 72 0.18

Benzo(b)fluoranthene314.8 172 14.8 172 12.0 141 1.6

Benzo(k)fluoranthene316.6 194 10.4 122 8.60 100 4.2

Benzo(a)pyrene 6.60 77 6.24 73 6.94 81 0.35

Indeno(1,2,3-cd)pyrene 5.45 64 6.16 72 5.37 63 0.43

Dibenz(a,h)anthracene 5.62 66 5.90 69 5.10 60 0.40

Benzo(g,h,i)perylene 6.15 72 6.41 75 6.50 76 0.18

1

 Three reagent water samples were spiked at 8.57μg/L with all target compounds (in acetone), 

and then extracted and analyzed by the method. A small spiking volume at high analyte 

concentration was used to maximize the analyte/water interaction prior to the extraction step. 

2

 Concentration units are μg/L. 

3

 High compound recovery was caused by an unidentified interference, possibly a silicone 

compound. 
SW-846 Update V 3511 - 10 

TABLE 2 

EXAMPLE MICROEXTRACTION GC/FID RECOVERY DATA FOR 

MAHs AND PAHs IN REAGENT WATER SPIKED AT 42.9 μg/L1

Compound 

Sample A Sample B Sample C Sample D Sample E 

Conc.2 % Rec. Conc.2 % Rec. Conc.2 % Rec. Conc.2 % Rec. Conc.2 % Rec. Co

Benzene 45.0 105 41.3 96 29.5 69 44.9 105 43.0 100 Toluene 44.5 104 45.8 107 43.9 102 45.4 106 46.0 107 Ethylbenzene 45.9 107 47.1 110 45.7 107 47.5 111 47.7 111 m/p-Xylene 92.3 108 95.1 111 91.9 107 95.3 111 95.7 112 Styrene 40.7 95 41.9 98 40.9 95 42.1 98 42.4 99 o-Xylene 49.6 116 51.2 120 49.3 115 50.8 119 51.3 120 1,2,4-Trimethylbenzene 44.0 103 45.9 107 44.8 104 45.6 106 45.4 106 Naphthalene 42.8 100 44.0 103 43.2 101 43.8 102 43.7 102 2-Methylnaphthalene 43.3 101 44.8 105 43.6 102 43.9 103 44.3 103 1-Methylnaphthalene 45.4 106 46.9 109 46.0 107 46.0 107 45.7 107 

Acenaphthylene 46.0 107 47.4 111 46.6 109 46.3 108 46.5 109 Acenaphthene 47.7 111 48.8 114 48.2 112 47.7 111 48.2 112 

Dibenzofuran 43.6 102 45.0 105 44.3 103 44.0 103 44.0 103 Fluorene 44.8 104 45.6 106 45.4 106 44.5 104 44.7 104 Phenanthrene 46.1 108 47.5 111 47.3 110 46.4 108 46.9 109 

Anthracene 37.4 87 38.6 90 38.4 90 38.0 89 37.7 88 

Fluoranthene 46.3 108 48.0 112 48.0 112 46.9 109 47.0 110 Pyrene 46.5 109 48.6 113 47.7 111 47.2 110 47.4 111 Benz(a)anthracene 41.9 98 44.8 105 44.3 103 42.8 100 43.0 100 Chrysene 42.8 100 44.8 105 44.1 103 43.5 102 43.9 102 Benzo(b)fluoranthene 47.2 110 50.6 118 49.8 116 46.9 109 48.4 113 Benzo(k)fluoranthene 52.2 122 50.5 118 46.8 109 46.9 109 47.5 111 Benzo(a)pyrene 39.2 91 41.3 96 40.7 95 40.0 93 40.0 93 Indeno(1,2,3-cd)pyrene 49.8 116 45.7 107 38.4 89 42.7 100 42.5 99 Dibenz(a,h)anthracene 35.4 83 36.7 86 35.3 82 35.5 83 35.4 83 Benzo(g,h,i)perylene 38.3 89 39.7 93 39.2 91 38.7 90 38.5 90 

1 Six reagent water samples were spiked at 42.9 μg/L with all target compounds (in acetone), and then extracted and analyzed by the method. A small 

concentration was used to maximize the analyte/water interaction prior to the extraction step. 2 Concentration units are μg/L. 
SW-846 Update V 3511 - 11 Revision 1 

October 2012 

TABLE 3 

EXAMPLE MICROEXTRACTION GC/FID RECOVERY DATA FOR 

MAHs AND PAHs IN REAGENT WATER SPIKED AT 857 μg/L1

Compound 

Sample A Sample B Sample C Std. 

Dev. 

Conc.2 % Rec. Conc.2 % Rec. Conc.2 % Rec. (Conc.2)

Benzene 819 96 866 101 797 93 35

Toluene 905 106 931 109 937 109 17

Ethylbenzene 922 108 933 109 978 114 30

m/p-Xylene 1840 107 1860 109 1950 114 59

Styrene 878 102 878 102 935 109 33

o-Xylene 946 110 951 111 998 116 28

1,2,4-Trimethylbenzene 933 109 928 108 991 116 35

Naphthalene 908 106 951 111 939 110 22

2-Methylnaphthalene 909 106 955 111 940 110 23

1-Methylnaphthalene 909 106 955 111 940 110 23

Acenaphthylene 905 106 962 112 937 109 29

Acenaphthene 913 107 958 112 945 110 23

Dibenzofuran 906 106 949 111 938 109 22

Fluorene 910 106 956 112 941 110 24

Phenanthrene 909 106 954 111 943 110 23

Anthracene 887 103 930 108 922 108 23

Fluoranthene 909 106 954 111 946 110 24

Pyrene 902 105 943 110 948 111 26

Benz(a)anthracene 907 106 947 110 942 110 22

Chrysene 937 109 992 116 968 113 28

Benzo(b)fluoranthene 894 104 875 102 930 108 28

Benzo(k)fluoranthene 924 108 1120 131 961 112 104

Benzo(a)pyrene 898 105 967 113 937 109 34

Indeno(1,2,3-cd)pyrene 895 104 942 110 933 109 25

Dibenz(a,h)anthracene 900 105 1010 118 941 110 56

Benzo(g,h,i)perylene 908 106 974 114 949 111 33

1

 Three reagent water samples were spiked at 857 μg/L with all target compounds (in acetone), 

and then extracted and analyzed by the method. A small spiking volume at high analyte 

concentration was used to maximize the analyte/water interaction prior to the extraction step. 

2 Concentration units are μg/L. 
SW-846 Update V 3511 - 12 Revision 1 

October 2012 

TABLE 4 

EXAMPLE MICROEXTRACTION GC/FID RECOVERY DATA FOR 

MAHs AND PAHs IN REAGENT WATER SPIKED AT 8570 μg/L1

Compound 

Sample A Sample B Sample C Std. 

Dev. 

Conc.2 % Rec. Conc.2 % Rec. Conc.2 % Rec. (Conc.2

)

Benzene 9470 111 8770 102 9070 106 351

Toluene 8440 98 8710 102 8510 99 140

Ethylbenzene 8750 102 8860 103 8860 103 64

m/p-Xylene 17500 102 17700 103 17700 103 115

Styrene NA NC NA NC NA NC NC

o-Xylene 8810 103 8910 104 8910 104 58

1,2,4-Trimethylbenzene 8840 103 8940 104 8950 104 61

Naphthalene 8520 99 8800 103 8480 99 174

2-Methylnaphthalene 8400 98 8880 104 8540 100 247

1-Methylnaphthalene 8420 98 8890 104 8540 100 244

Acenaphthylene 8490 99 8750 102 8440 98 167

Acenaphthene 8520 99 8790 103 8470 99 172

Dibenzofuran 8450 99 8930 104 8600 100 246

Fluorene 8550 100 8820 103 8510 99 169

Phenanthrene 8680 101 8940 104 8640 101 163

Anthracene 8230 96 8480 99 8150 95 172

Fluoranthene 8560 100 8820 103 8520 99 163

Pyrene 8630 101 8910 104 8600 100 171

Benz(a)anthracene 8630 101 8890 104 8610 100 156

Chrysene 8450 99 8750 102 8400 98 189

Benzo(b)fluoranthene 8850 103 9110 106 8810 103 163

Benzo(k)fluoranthene 8420 98 8660 101 8380 98 151

Benzo(a)pyrene 8700 102 8960 105 8660 101 163

Indeno(1,2,3-cd)pyrene 9480 111 9670 113 9480 111 110

Dibenz(a,h)anthracene 8550 100 8970 105 8540 100 245

Benzo(g,h,i)perylene 8990 105 9310 109 9030 105 174

NA = Not available 

NC = Not calculated 

1

 Three reagent water samples were spiked at 8570 μg/L with all target compounds (in 

acetone), and then extracted and analyzed by the method. A small spiking volume at high 

analyte concentration was used to maximize the analyte/water interaction prior to the 

extraction step. 

2 Concentration units are μg/L. 
SW-846 Update V 3511 - 13 Revision 1 

October 2012 

Appendix A: 

Summary of Revisions to Method 3511 (as compared to previous Revision 0, November 2002)

1. Improved overall method formatting for consistency with new SW-846 methods style 

guidance. The format was updated to Microsoft Word 2007.docx. 

2. Minor editorial and technical revisions were made throughout to improve method clarity. 

3. The revision number was changed to1 and the date published was changed to May 2012. 

4. This appendix was added showing changes from the previous revision. 

5. Added Updated IDP language and LLOQ verification standard language to Secs. 9.2 and 

9.3. 

6. Added a reference in Sec. 16.